Classifications

• • C—CHEMISTRY; METALLURGY
  • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
  • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
  • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
  • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
  • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
  • C04B35/571—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained from Si-containing polymer precursors or organosilicon monomers
• • C—CHEMISTRY; METALLURGY
  • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
  • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
  • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/71—Ceramic products containing macroscopic reinforcing agents
  • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
  • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T428/00—Stock material or miscellaneous articles
  • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
  • Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T428/00—Stock material or miscellaneous articles
  • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
  • Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
  • Y10T428/264—Up to 3 mils
  • Y10T428/265—1 mil or less
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T428/00—Stock material or miscellaneous articles
  • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
  • Y10T428/2913—Rod, strand, filament or fiber
  • Y10T428/2916—Rod, strand, filament or fiber including boron or compound thereof [not as steel]
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T428/00—Stock material or miscellaneous articles
  • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
  • Y10T428/2913—Rod, strand, filament or fiber
  • Y10T428/2918—Rod, strand, filament or fiber including free carbon or carbide or therewith [not as steel]
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T428/00—Stock material or miscellaneous articles
  • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
  • Y10T428/2913—Rod, strand, filament or fiber
  • Y10T428/2933—Coated or with bond, impregnation or core
  • Y10T428/2938—Coating on discrete and individual rods, strands or filaments
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T428/00—Stock material or miscellaneous articles
  • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
  • Y10T428/2913—Rod, strand, filament or fiber
  • Y10T428/2933—Coated or with bond, impregnation or core
  • Y10T428/294—Coated or with bond, impregnation or core including metal or compound thereof [excluding glass, ceramic and asbestos]
  • Y10T428/2942—Plural coatings
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T428/00—Stock material or miscellaneous articles
  • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
  • Y10T428/2913—Rod, strand, filament or fiber
  • Y10T428/2933—Coated or with bond, impregnation or core
  • Y10T428/294—Coated or with bond, impregnation or core including metal or compound thereof [excluding glass, ceramic and asbestos]
  • Y10T428/2942—Plural coatings
  • Y10T428/2949—Glass, ceramic or metal oxide in coating
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T428/00—Stock material or miscellaneous articles
  • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
  • Y10T428/2913—Rod, strand, filament or fiber
  • Y10T428/2973—Particular cross section
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T428/00—Stock material or miscellaneous articles
  • Y10T428/30—Self-sustaining carbon mass or layer with impregnant or other layer
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
  • Y10T442/60—Nonwoven fabric [i.e., nonwoven strand or fiber material]
  • Y10T442/608—Including strand or fiber material which is of specific structural definition
  • Y10T442/614—Strand or fiber material specified as having microdimensions [i.e., microfiber]

Definitions

• thermostructural Composite Articles and Method for Making Same FIELD OF THE INVENTION This invention relates to thermostructural composite articles and to methods of fabricating such articles.
• thermostructural composite articles i.e., articles of composite materials which exhibit not only high strength but which also maintain their strength at elevated temperatures and/or in harsh conditions
• thermostructural composite article comprises a refractory matrix reinforced with silicon carbide fiber such as the composites disclosed in U.S. Patent Nos. 4,752,503 and 5,026,604.
• Composites of a refractory material reinforced with silicon carbide fiber are typically made by fabricating a preform of the fiber and subsequently forming a matrix about the fibers in the fiber preform.
• a particularly desirable technique for forming the matrix uses a process referred to as chemical vapor infiltration (CVI) in which precursor gases are passed into and through the pores in the preform under conditions such that the desired matrix is deposited.
• CVI chemical vapor infiltration
• known refractory matrix/silicon carbide fiber reinforced composite articles of this type have very desirable properties, composite articles with increased strength and/or toughness are desired for some applications which require withstanding more severe conditions or to improve the margin of safety in existing applications.
• the invention provides a thermostructural composite article and a method for making the article.
• the article comprises silicon carbide reinforcing fibers having an oxygen content by weight of not more than about 14% and an average diameter of less than about 20 microns in a refractory matrix at least partially formed by chemical vapor infiltration.
• the fibers in the composite article of the invention have an end-to-end fiber diameter uniformity ratio of less than about 1.5.
• the matrix is selected from the class consisting of carbides, nitrides, oxides, and carbon.
• the matrix is selected from the class consisting of SiC, HfC, Si3N , BN, AI2O3, Zr ⁇ 2, Ta 2 Oj, 1O2 HfB 2 and pyrolitic carbon and most preferably comprises SiC.
• the thermostructural composite article further includes at least one interfacial layer of a refractory material between the fibers and the matrix, the layer adhering to the fibers and the matrix and being capable of elastic deformation in shear.
• the interfacial layer is selected from the class consisting of pyrolitic carbon, carbides, nitrides, and oxides.
• the fibers are exposed to chemical treatment prior to formation of the matrix.
• the chemical treatment includes the step of contacting the fibers with a hydrofluoric acid solution.
• fibers of the composite article include an oxygen-scavenging sealant forming region provided by a discontinuous particulate material containing a B 2 O 3 glass precursor.
• At least a portion of the matrix of the composite article is formed by in situ reaction of a matrix precursor.
• an external protective coating of a refractory material is provided on the composite article.
• the invention provides a refractory matrix silicon carbide fiber reinforced composite with improved mechanical properties including tensile strength and breaking elongation. The improvements are realized over a wide range of temperatures.
• Curve A is graphical representation of tensile stress plotted against elongation at ambient temperature for a composite in accordance with the invention prepared as described in Example 1; Curve B represents the same behavior for a comparative composite (Comparative 1);
• Figure 2 is an optical micrographs at 1000X of a polished cross-section of the composite in accordance with the invention prepared in accordance with the procedures of Example 1 from which the end-to-end fiber uniformity ratio can be measured;
• Figure 3 is an optical micrograph as in Figure 2 of a comparative composite (Comparative 1);
• Figure 4 is an optical micrograph as in Figure 2 of a comparative composite (Comparative 2);
• Curve C is graphical representation of tensile stress plotted against elongation at 1000°C in nitrogen for a composite in accordance with the invention prepared as described in Example 2; Curve D represents the same behavior for a comparative composite (Comparative 1); and
• Figure 6 is a graphical representation similar to Figure 5 for the same composites at 1200°C in nitrogen.
• the silicon carbide reinforcing fibers used in accordance with the invention are of the type which have an oxygen content by weight of not more than about 14% and an average diameter of less than about 20 microns.
• the fibers have an end-to-end fiber diameter uniformity ratio of less than about 1.5.
• An end-to-end fiber diameter uniformity ratio of less than about 1.5 means that the ratio of the diameter of the largest fiber to the diameter of the smallest fiber when the fibers are viewed in cross-sectional optical micrographs is less than about 1.5.
• the term silicon carbide reinforcing fiber is not intended to exclude the presence of other elements in addition to oxygen.
• the silicon carbide fiber has a titanium content by weight of about 0.1 to about 5%.
• thermostructural composite article is made by fabrication of a reinforcing preform of the silicon carbide fibers prior to the formation of the matrix by chemical vapor infiltration (CVI).
• a typical fiberous preform has a nominal fiber volume of 25-50 % of silicon carbide fibers. The fibers are arranged in bundles or tows, typically containing 200, 400, 800, or 1600 fibers or filaments.
• the fiber tows can be woven into a fabric of various weave architectures, such as plain-weave, 5 or 8 harness-satin weaves, or angle-interlock 3D weaves.
• weave architectures such as plain-weave, 5 or 8 harness-satin weaves, or angle-interlock 3D weaves.
• one or more layers of fabric are assembled, usually in a stacking arrangement, to form a fiberous preform that has a nominal fiber volume of 25-50%, with the balance being voids.
• braiding or filament winding techniques can be used to produce a 2D, 3D or 4D preform architecture.
• a tool such as one made of graphite or other material that does not adversely effect further processing, can be employed to help maintain the shape of the fiberous preform for subsequent processing steps.
• a dimensional stabilizing resin such as poly-methyl-methacrylate or phenolic, can be utilized to rigidize the preform in preparation for subsequent processing.
• the fibers are advantageously exposed to chemical treatment prior to formation of the matrix.
• the chemical treatment includes the step of contacting the fibers with a hydrofluoric acid solution.
• the interfacial layer is a refractory material which adheres to the fibers and the matrix and which is capable of elastic deformation in shear.
• the interfacial layer is selected from the class consisting of pyrolitic carbon, carbides, nitrides, and oxides.
• the material of the interfacial layer is different from one or both of the matrix and fiber.
• the interfacial layer is preferably applied by CNI using known techniques such as those disclosed in U.S. Patent ⁇ os. 4,752,503 and 5,026,604.
• CNI processing can be used to form a pyrolytic carbon interfacial layer around fibers.
• the formation of a pyrolytic carbon layer can be accomplished by passing a carbon containing gas (methane, propane, propylene, butane, pentane, hexane etc.) over the preform at elevated temperature ( ⁇ 1000°C) and reduced pressure. Under these conditions, the carbon containing gas diffuses into the preform and deposits a thin layer of solid pyrolytic carbon on the surfaces of the fibers.
• a carbon containing gas methane, propane, propylene, butane, pentane, hexane etc.
• Desirable coating thicknesses range from 40 nanometers (nm) to 1000 nm (1 micron), and the preferable range is between 60 nm and 300 nm.
• an oxygen-scavenging sealant forming region provided by a discontinuous particulate material containing a B 2 O3 glass precursor on the fibers of the composite article.
• This region can be formed before or after the formation of the interfacial layer and can improve the resistance of the composite to oxidation.
• the techniques disclosed in U.S. Patent No. 5,094,901 are useful for this purpose.
• a refractory matrix is formed about the reinforcing fibers.
• the refractory matrix is at least partially formed by chemical vapor infiltration (CNI).
• the refractory matrix is preferably selected from the class consisting of carbides, nitrides, oxides, and carbon. More preferably, the matrix is selected from the class consisting of SiC, HfC, Si 3 ⁇ 4 , BN, Al 2 O 3 , ZrO 2 , Ta 2 O 5 , TiO 2 HfB 2 and pyrolitic carbon and most preferably comprises SiC. It will be understood that the preferred matrix materials may be the pure compositions represented by the chemical formulas above or may be modified to include minor quantities of other elements.
• CVI CVI
• An isothermal CNI process is preferred but a forced-flow CNI process could also be used.
• CNI can be carried out by passing appropriate precursor gases, such as methyl-trichloro- silane (MTS) or dimethyl-dichloro-silane (DDS) or a combination of silane and a hydrocarbon gas, e.g. methane, propane, propylene over the preform.
• precursor gases such as methyl-trichloro- silane (MTS) or dimethyl-dichloro-silane (DDS) or a combination of silane and a hydrocarbon gas, e.g. methane, propane, propylene over the preform.
• MTS methyl-trichloro- silane
• DDS dimethyl-dichloro-silane
• hydrocarbon gas e.g. methane, propane, propylene
• residual porosity in the final composite article is not mandatory, it is usually desirable to leave some residual porosity in the final composite, typically 5 to 20%, to reduce brittle behavior. If desired, machining can be employed at some point in the formation of the matrix to refine the shape the composite article or to remove a surface seal coating for further processing.
• polycarbosilane or phenolic resin can be used to form SiC and carbon matrices, respectively, by heating the preform coated with the resins at temperatures above the decomposition temperature of the resins.
• additional processing can be employed to apply additional coatings to the composite article after matrix formation to enhance the performance in oxidizing, corrosive, erosive or other harsh environments.
• Chemical vapor deposition (CVD) is a known technique which can be used to apply coatings of this type.
• the enhanced strength of the composite articles in accordance with the invention offers increased thermomechanical performance in use and, due to the improved elongation, also provides better margins of safety similar to the effect provided by the plasticizing of metals.
• Example 1 Composite a 800 filament silicon carbide fiber tow, sold under the trademark LOX-M TYRANNO by Ube Industries, Ltd., Japan, is woven into a balanced plain-weave fabric. Layers of the fabric are cut and stacked into a preform with fibers orientated in two dimensions within the plane. The stacked layers of fabric are compacted to obtain a fiber volume of forty percent, nominal, in the preform. In this example, eight plys are used to produce a plate geometry with a two millimeter thickness and a forty percent fiber volume, nominal.
• the nominal forty percent fiber volume is chosen so that the volume of reinforcing fibers in the final composite article would be directly comparable in evaluation to thermomechanical properties of known composites made with a forty percent by volume of silicon carbide fibers sold under the trademark NICALON 202 by Nippon Carbon Co., Japan.
• Table 1 shows that the tensile properties of LOX-M TYRANNO silicon carbide fibers as reported by the producer are very similar to those for NICALON 202 silicon carbide fibers.
• Silicon carbide fibers reported as having twenty-five weight percent oxygen content are also sold by Ube Industries as standard grade (Grade D) TYRANNO by trademark and the properties of this fiber are also included in Table 1 for comparative purposes.
• a thin pyrolytic carbon (-0.1 microns) interfacial layer is applied to the fibers of the preform using a chemical vapor infiltration process of the type described in U. S. Patent No. 4,752,503.
• a SiC matrix is formed on fiber of the preform using chemical vapor infiltration process of the type described in U. S. Patent No. 4,752,503 using apparatus as disclosed in U. S. Patent 4,823,734. SiC is formed between the coated fibers until a final porosity of 5-20% is achieved in the composite article.
• the resulting composite articles have final bulk densities of 2.2 to 2.6 g/cc.
• Comparative Composite 2 denotes composite article coupons made with standard grade TYRANNO reinforcing fibers.
• Figure 1 illustrates the behavior of the Example 1 Composite article coupons (Curve A) under tensile loading at ambient temperature in terms of the pulling force (tensile stress) and the measured elongation.
• the second curve B is also shown in Figure 1 that represents the tensile behavior of the Comparative 1 Composite article coupons.
• Table 2 it is found that the Example 1 Composite article coupons possess, on the average, a 57% increase in tensile strength and a 141% increase in elongation in comparison with the Comparative 1 Composite coupons.
• Comparative 2 Composite articles that are reinforced with standard-grade TYRANNO fibers the composite articles made with LOX-M TYRANNO fibers possess significantly higher tensile strengths and elongations even though the fiber strengths are equivalent.
• FIG. 2 is an optical micrograph at 1000X magnification of a polished cross-section of the composite of the invention from which the end-to-end fiber uniformity ratio can be measured. Using a ruler on the micrograph of Figure 2, measuring the largest fiber diameter and the smallest fiber diameter results in an end-to-end fiber uniformity ratio of about 1.2.
• Figure 3 is a similar optical micrograph of Comparative 1 composite article which shows that the end-to-end fiber uniformity ratio of the comparative composite is about three.
• Figure 4 is a similar optical micrograph of the Comparative 2 composite article that has been etched. Figure 4 shows that the end-to-end fiber uniformity ratio is 1.8.
• Example 2 To prepare another composite article in accordance with the invention (Example 2 Composite), the same fiber and procedures as in Example 1 are used except that the tow contains 400 filaments per fiber tow. Due to the decreased number of fibers in the tow, 22 plys of the balanced plain- weave fabric were used to make the three millimeter thick preform, again with a forty percent, nominal fiber volume.
• Example 2 composite and Comparative 1 composite articles were summarized in Table 3.
• Example 3 Composite To prepare another composite article in accordance with the invention (Example 3 Composite), the same fiber and procedures as in Examples 1 and 2 are used except that the tow contains 800 filaments per fiber tow. 14 plys of the balanced plain-weave fabric were used to make the three millimeter thick preform, again with a forty percent, nominal fiber volume.
• Example 3 composite coupons were tensile tested as in Example 1. At ambient temperature, the tensile behaviour of Example 3 composite coupons is similar to that observed for Example 1 composite coupons, illustrated in Figure 1. The tensile test results for Example 3 composite articles and Comparative 1 composite articles (from Example 1) are summarized in Table 4. TABLE 4

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• 1994
  • 1994-01-06 WO PCT/US1994/000071 patent/WO1994015887A1/fr not_active Ceased
  • 1994-01-06 EP EP94907139A patent/EP0678083B1/fr not_active Expired - Lifetime
  • 1994-01-06 JP JP6516146A patent/JPH08505355A/ja active Pending
  • 1994-01-06 DE DE69402827T patent/DE69402827T2/de not_active Expired - Fee Related
  • 1994-01-06 CA CA002153667A patent/CA2153667A1/fr not_active Abandoned
  • 1994-01-06 AU AU60823/94A patent/AU6082394A/en not_active Abandoned
• 1995
  • 1995-08-25 US US08/519,861 patent/US5733655A/en not_active Expired - Fee Related

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